DD273442A5 - METHOD FOR OBTAINING STEVIOSIDES FROM PLANT RAW MATERIAL - Google Patents
METHOD FOR OBTAINING STEVIOSIDES FROM PLANT RAW MATERIAL Download PDFInfo
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- DD273442A5 DD273442A5 DD88318081A DD31808188A DD273442A5 DD 273442 A5 DD273442 A5 DD 273442A5 DD 88318081 A DD88318081 A DD 88318081A DD 31808188 A DD31808188 A DD 31808188A DD 273442 A5 DD273442 A5 DD 273442A5
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- ion exchange
- exchange resin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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- Health & Medical Sciences (AREA)
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- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Alternative & Traditional Medicine (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Saccharide Compounds (AREA)
- Seasonings (AREA)
- Outer Garments And Coats (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Gloves (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
Description
Die Erfindung richtet sich auf ein Verfahren zur Gewinnung von Steviosiden aus getrocknetem pflanzlichem Rohmaterial von Stevia rebaudiana Bertoni unter Extraktion und Reinigung, wobei durch chemische Behandlung unerwünschte Verunreinigungen entfernt und die Reinigung durch eino Behandlung mittels Anion- und Kation-Austauschorharzen erfoigt.The invention is directed to a process for recovering steviosides from dried vegetable raw material from Stevia rebaudiana Bertoni under extraction and purification whereby chemical treatment removes undesirable contaminants and performs purification by treatment with anion and cation exchange resins.
Stevioside werden als brauchbare künstliche Süßstoffe verwendet und kalorienarmen Nahrungsmitteln zugesetzt oder als Ersatz für natürlichen Zucker gebracht. Künstliche Süßstoffe wurden entwickelt zum Gebrauch für Diabetiker und zur Verminderung des Kaloriengehalts von Nahrungsmittelzubereitungen, insbesondere für eine kalorienarme Diät. Diese Süßstoffe sind vielfach süßer als der natürliche Zucker und können, um das gleiche Maß an Süßwirkung zu erzielen, in geringen Mengen verwendet werden. Zahlreiche Süßstoffe sind synthetischer Natur, wie z. B. Saccharin, Cyclamate und Aspartame. Einige hiervon sind verboten oder in ihrem Gebrauch eingeschränkt, weil pharmakotogische Untersuchungen ergeben haben, daß sie Krebs erzeugen können. Die Stevioside dagegen sind voll verwendbar und haLün in klinischen Tests keine nachteiligen Wirkungen gezeigt.Steviosides are used as useful artificial sweeteners and added to low-calorie foods or substituted for natural sugars. Artificial sweeteners have been developed for use by diabetics and to reduce the calorie content of food preparations, especially for a low calorie diet. These sweeteners are often sweeter than the natural sugar and can be used in small amounts to achieve the same level of sweetness. Many sweeteners are synthetic in nature, such as. For example, saccharin, cyclamates and aspartame. Some of these are banned or limited in use because pharmacokinetic studies have shown that they can cause cancer. The steviosides, however, are fully usable and have not shown any adverse effects in clinical tests.
Gebräuchliche Verfahren zur Extraktion und Reinigung von Stevi osiden sind fast ausschließlich verbunden mit der Verwendung organischer Lösungsmittel, wie Methanol, Äthanol oder Äther, und viele erfordern zunächst die Absorption der Stevioside an ein Harz unter nachfolgender Elution mit einem organischen Lösungsmittel. Die aus diesem Verfahren konzentrierten eingedickten Lösungen werden üblicherweise mit Methanol oder Äthanol behandelt, um die schließliche Kristallisation des Endgemisches zu erreichen. Andere Verfahren bedienen sich Eisen· oder Aluminiumsalze, um Verunreinigungen zu entfernen. Diese beiden Mittel erfordern eine weitere Behandlung mit Natriumhydroxid zur Entfernung von Resten der Eisen- oder Aluminiumsalze.Common methods for extracting and purifying steviosides are almost exclusively associated with the use of organic solvents, such as methanol, ethanol or ether, and many require the absorption of the steviosides onto a resin, followed by elution with an organic solvent. The thickened solutions concentrated from this process are usually treated with methanol or ethanol to achieve the final crystallization of the final mixture. Other processes use iron or aluminum salts to remove impurities. These two agents require further treatment with sodium hydroxide to remove residues of the iron or aluminum salts.
Mit der Erfindung wird ein Verfahren zur Gewinnung von Steviosiden zur Verfügung gestellt, das gegenüber den bekannten Verfahren vereinfacht, kostengünstiger und zu besseren Ergebnissen führt.The invention provides a process for the production of steviosides which, compared with the known processes, simplifies, reduces costs and leads to better results.
Die Aufgabe der Erfindung besteht darin, ein verbessertes Verfahren zur Gewinnung von Steviosiden bereitzustelle.). Bei dem erfindungsgemäßen Verfahren besteht das einzige chemische Additiv aus einem Zusatz von Calciumhydroxid zum Ausgangsmaterial, wodurch die Masse der unerwünschten Verunreinigungen und Farbstoffe entfernt wird. Alle weiterenThe object of the invention is to provide an improved method for the production of steviosides.). In the method according to the invention, the sole chemical additive consists of an addition of calcium hydroxide to the starting material, whereby the mass of undesired impurities and dyes is removed. All further
Vorfahronsschriuo werden mit Wasser als Lösungsmittel ausgeführt, und das Ergebnis wird durch Verdampfung des Wassors und Trocknung gewonnon als ein Stoviosid von hoher Reinheit, gutom Geschmack und einwandfreier Färbung sowie mit oinor hohen Oosnmtausböuto gegenüber dom Rohmaterial. DIo Erfindung besteht darin, daß bol einem Vorfahren der eingangs bezeichneten Art durch Behandlung in Wasser bei Temperaturen zwischen Raumtemperatur und 650C und untor Rühren sowio anschließender Filtration oder Zentrifugieren oin Extrakt gewonnen und diesor mit Ca(OH)2 bohandolt wird, worauf mittels Filtration oder Zentrifugieren oin Niederschlag gewonnon unH mit oinom stark sauron lononaustauschorharz und anschließend mit einem schwach basischen lonenaustauschorharz behandelt, gefiltert und getrocknet wird. Als saure Ionenaustauscher kommen die untor dem Handelsnamen Domex 50 W, Rohm und Haas IRA120 oder wirkungsgleiche Harze in Betracht. Dio basischen Ionenaustauscherharze können beispielsweise die unter dem Handelsnamen Domex WGR, Domex MWA-1, Rohm und Hap 3IR4B oder Rohm und Hass IRA93 bekannten oder wirkungsgleiche Harze sein. Die Lösung wird durch ein feines Filtersystem geführt und eine Probe zur Ermittlung der Reinheit und Qualität vordampft. Entsprechend der gewünschten Reinheit und Qualität des Endprodukts kann dieses Verfahren einschließlich der Anwendung der stark sauren Ionenaustauscherharze und der schwachen basischen Ionenaustauscherharze mehrfach, im allgemeinen bis dreifach, wiederholt worden. DIo Lösung wird dann konzentriert und gefiltert. Das Filtrat wird getrocknet, und es wird ein weißes Pulver gewonnen, welches etwa 75% Steviosid-Verbindungen enthält.Process silica are carried out with water as a solvent, and the result is obtained by evaporation of the water and drying as a stovioside of high purity, good taste, and perfect coloration, as well as high osmosis effluvium over raw material. DIo invention is that bol an ancestor of the type described by treatment in water at temperatures between room temperature and 65 0 C and untori stirring sowio subsequent filtration or centrifugation oin extract recovered and isor with bo (Bo) 2 with potassium (OH) 2 , followed by filtration or centrifugation or precipitate, but not otherwise, with a strongly acid ion exchange resin and then treated with a weakly basic ion exchange resin, filtered and dried. Suitable acidic ion exchangers are those which are not covered by the trade names Domex 50 W, Rohm and Haas IRA120 or the same type of resins. Dio basic ion exchange resins may be, for example, the resins known or equivalent under the trade names Domex WGR, Domex MWA-1, Rohm and Hap 3IR4B or Rohm and Hass IRA93. The solution is passed through a fine filter system and a sample pre-evaporated to determine the purity and quality. Depending on the desired purity and quality of the final product, this process, including the use of the strongly acidic ion exchange resins and the weak basic ion exchange resins, can be repeated several times, generally up to three times. The solution is then concentrated and filtered. The filtrate is dried and a white powder is obtained containing about 75% stevioside compounds.
Es liegt im Rahmen der Erfindung, daß der Extrakt zur Bildung des Niederschlags mit Calciumoxid, Calciumcarbonat oder anderen basischen Calciumsalzen behandelt wird. Eine andere Alternative hierzu bildet die Behandlung dos Extraktes zur Bildung dos Niederschlags mit basischen Salzen des Magnesiums oder Aluminiums. Vorteilhafterweiso werden die basischen Salze während der Extraktion und unter Rühren dem Wasser zugesetzt.It is within the scope of the invention that the extract is treated to form the precipitate with calcium oxide, calcium carbonate or other basic calcium salts. Another alternative to this is the treatment of the extract to form the precipitate with basic salts of magnesium or aluminum. Advantageously, the basic salts are added to the water during extraction and with stirring.
Schließlich sieht die Erfindung vor, daß nach Behandlung mit dom stark sauren lononaustauscherharz und einem schwachen basischen lonenaustauscherharz das gewonnene Filtrat mit einem stark sauren lononaustauschorharz sowie anschließend einem starken basischen lonenaustauschorharz behandelt und die gewonnene Lösung konzentriert, gefiltert und getrocknet wirdFinally, the invention contemplates that after treatment with dom ion exchange resin and a weak basic ion exchange resin, the recovered filtrate is treated with a strongly acidic ion exchange resin and then a strong basic ion exchange resin and the recovered solution is concentrated, filtered and dried
Das erfindungsgemäße Vorfahren wird anhand der folgenden Beispiele im einzelnen erläutert: The ancestor according to the invention is explained in detail with reference to the following examples:
BeisploM:BeisploM:
Das Rohmaterial, welches die Stevioside enthält, wird durch Wasserextraktion aus einem Kilogramm Pflanzenmaterial bei Temperaturen in der Größenordnung von Raumtemperatur bis 65°C gewonnon. Ohne zusätzliche Konzentration wird dieser Extrakt mit Calciumhydroxid behandelt, um eine Anzahl unerwünschter Pflanzenbestandteile zu entfernen, urd das Ganze wird in einem feinen Filtorsystom filtriert. Das Ergebnis ist eine klare Lösung, die 279 Gramm Roh-Stevioside enthält. Diese klare Lösung wird dann mit einem stark sauren lonenaustauscherharz, wie z. B. Dowes 5OW, behandelt und das gewonnene Eluat dann mit einem schwachen basischen lonenaustauscherharz, wie z. B. Domex WGR od. dgl. behandelt. Das aus diesor Behandlung hervor/>dhende Eluat wird gefiltert durch ein feines Filtermedium, bevor der nächste Verfahrensschritt folgt. Die Aufeinanderfolge der Behandlungen mit stark saurem Harz und schwachem basischem Harz wird so lange wiederholt, bis oin befriedigendes Produkt erlangt wird. Dies kann sich von einer bis zur fünfmaligen Behandlung erstrecken. Nach der Elution und Filtration am Ende der letzten lonenaustauschorbehandlung wird das gewonnene Eluat konzentriert und in einem feinen Filtersystem gefiltert. Das Filtrat wird getrocknet und ergibt ein gereinigtes Produkt mit 107 Gramm von etwa 75% reinen Stoviosiden.The raw material containing the steviosides is obtained by water extraction from one kilogram of plant material at temperatures of the order of room temperature to 65 ° C. Without additional concentration, this extract is treated with calcium hydroxide to remove a number of undesired plant constituents, and the whole is filtered in a fine filter system. The result is a clear solution that contains 279 grams of raw stevioside. This clear solution is then treated with a strongly acidic ion exchange resin, such. B. Dowes 5OW, treated and the recovered eluate then with a weak basic ion exchange resin, such as. B. Domex WGR od. Like. Treated. The eluate resulting from this treatment is filtered through a fine filter medium before the next process step follows. The sequence of treatments with strong acid resin and weak basic resin is repeated until satisfactory product is obtained. This can range from one to five treatments. After elution and filtration at the end of the last ion exchange treatment, the recovered eluate is concentrated and filtered in a fine filtration system. The filtrate is dried to give a purified product with 107 grams of about 75% pure stoviosides.
Dieses Verfahren entspricht im wesentlichen dem Beispiel 1, jedoch wird das Eluat nach dreifach aufeinanderfolgender Behandlung mit einem stark sauren Harz und einem schwachen basischen Harz und Filtration konzentriert. Das Konzentrat wird dann ein weiteres Mal mit einem entsprechend starken sauron Harz und anschließend mit einem stark basischen Harz, wie z. B. Dowex 2-X oder Rohm und Haas IRA410 od. dgl. behandelt. Das Ergebnis dieser Behandlung wird dann konzentriert und das Konzentrat in einem Feinfiltersystem gefiltert. Oas Endprodukt gewinnt man durch Trocknen, es ergibt 102 Grammeines gereinigten Erzeugnisses, welches etwa 75% reine Stevioside enthält, jedoch weniger bitter bei der Geschmacksprüfung ist.This procedure is essentially the same as Example 1 except that the eluate is concentrated after treatment with a strong acid resin and a weak basic resin and filtration three times in succession. The concentrate is then once more with a correspondingly strong sauron resin and then with a strong base resin such. B. Dowex 2-X or Rohm and Haas IRA410 od. Like. Treated. The result of this treatment is then concentrated and the concentrate filtered in a fine filter system. The final product is obtained by drying, giving 102 grams of a purified product containing about 75% pure steviosides but less bitter in the taste test.
Claims (7)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP87110541A EP0302948B1 (en) | 1987-07-21 | 1987-07-21 | Process for obtaining steviosides from plants |
Publications (1)
Publication Number | Publication Date |
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DD273442A5 true DD273442A5 (en) | 1989-11-15 |
Family
ID=8197144
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DD88318081A DD273442A5 (en) | 1987-07-21 | 1988-07-19 | METHOD FOR OBTAINING STEVIOSIDES FROM PLANT RAW MATERIAL |
Country Status (17)
Country | Link |
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US (1) | US4892938A (en) |
EP (1) | EP0302948B1 (en) |
JP (1) | JPH01131191A (en) |
CN (1) | CN1021826C (en) |
AT (1) | ATE97910T1 (en) |
AU (1) | AU609154B2 (en) |
CA (1) | CA1310963C (en) |
DD (1) | DD273442A5 (en) |
DE (1) | DE3788351D1 (en) |
DK (1) | DK406188A (en) |
ES (1) | ES2046979T3 (en) |
IE (1) | IE63706B1 (en) |
IN (1) | IN171592B (en) |
NO (1) | NO173913C (en) |
NZ (1) | NZ225471A (en) |
SU (1) | SU1834646A3 (en) |
ZA (1) | ZA885176B (en) |
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JPS5139239B2 (en) * | 1973-06-29 | 1976-10-26 | ||
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-
1987
- 1987-07-21 AT AT87110541T patent/ATE97910T1/en not_active IP Right Cessation
- 1987-07-21 EP EP87110541A patent/EP0302948B1/en not_active Expired - Lifetime
- 1987-07-21 DE DE87110541T patent/DE3788351D1/en not_active Expired - Fee Related
- 1987-07-21 ES ES87110541T patent/ES2046979T3/en not_active Expired - Lifetime
-
1988
- 1988-07-11 CA CA000571680A patent/CA1310963C/en not_active Expired - Lifetime
- 1988-07-15 IN IN498/MAS/88A patent/IN171592B/en unknown
- 1988-07-18 ZA ZA885176A patent/ZA885176B/en unknown
- 1988-07-19 NZ NZ225471A patent/NZ225471A/en unknown
- 1988-07-19 DD DD88318081A patent/DD273442A5/en not_active IP Right Cessation
- 1988-07-20 IE IE221388A patent/IE63706B1/en not_active IP Right Cessation
- 1988-07-20 DK DK406188A patent/DK406188A/en not_active Application Discontinuation
- 1988-07-20 SU SU884356128A patent/SU1834646A3/en active
- 1988-07-20 US US07/221,811 patent/US4892938A/en not_active Expired - Fee Related
- 1988-07-20 AU AU19219/88A patent/AU609154B2/en not_active Ceased
- 1988-07-21 CN CN88104468A patent/CN1021826C/en not_active Expired - Fee Related
- 1988-07-21 JP JP63180435A patent/JPH01131191A/en active Pending
- 1988-08-01 NO NO883234A patent/NO173913C/en unknown
Also Published As
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ZA885176B (en) | 1989-04-26 |
NO883234L (en) | 1989-02-13 |
EP0302948B1 (en) | 1993-12-01 |
IE882213L (en) | 1989-01-21 |
EP0302948A3 (en) | 1989-03-22 |
ATE97910T1 (en) | 1993-12-15 |
SU1834646A3 (en) | 1993-08-15 |
CN1030762A (en) | 1989-02-01 |
DK406188A (en) | 1989-01-22 |
CN1021826C (en) | 1993-08-18 |
NO173913C (en) | 1994-02-23 |
AU609154B2 (en) | 1991-04-26 |
DK406188D0 (en) | 1988-07-20 |
ES2046979T3 (en) | 1994-02-16 |
IN171592B (en) | 1992-11-21 |
IE63706B1 (en) | 1995-05-31 |
JPH01131191A (en) | 1989-05-24 |
NZ225471A (en) | 1991-02-26 |
NO883234D0 (en) | 1988-07-20 |
CA1310963C (en) | 1992-12-01 |
NO173913B (en) | 1993-11-15 |
US4892938A (en) | 1990-01-09 |
DE3788351D1 (en) | 1994-01-13 |
EP0302948A2 (en) | 1989-02-15 |
AU1921988A (en) | 1989-01-27 |
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